US20230051424A1 - Process for the preparation of a dental restoration - Google Patents

Process for the preparation of a dental restoration Download PDF

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Publication number
US20230051424A1
US20230051424A1 US17/819,812 US202217819812A US2023051424A1 US 20230051424 A1 US20230051424 A1 US 20230051424A1 US 202217819812 A US202217819812 A US 202217819812A US 2023051424 A1 US2023051424 A1 US 2023051424A1
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US
United States
Prior art keywords
process according
ceramic material
cooling
oxide ceramic
cooling rate
Prior art date
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Pending
Application number
US17/819,812
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English (en)
Inventor
Corina Serban
Frank Rothbrust
Christian Ritzberger
Sebastian Krolikowski
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Ivoclar Vivadent AG
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Ivoclar Vivadent AG
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Filing date
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Application filed by Ivoclar Vivadent AG filed Critical Ivoclar Vivadent AG
Publication of US20230051424A1 publication Critical patent/US20230051424A1/en
Assigned to IVOCLAR VIVADENT AG reassignment IVOCLAR VIVADENT AG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: Krolikowski, Sebastian, RITZBERGER, CHRISTIAN, ROTHBRUST, FRANK, SERBAN, CORINA
Pending legal-status Critical Current

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
    • A61C13/0003—Making bridge-work, inlays, implants or the like
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
    • A61C13/08—Artificial teeth; Making same
    • A61C13/083—Porcelain or ceramic teeth
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C5/00—Filling or capping teeth
    • A61C5/70—Tooth crowns; Making thereof
    • A61C5/77—Methods or devices for making crowns
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/70—Preparations for dentistry comprising inorganic additives
    • A61K6/78—Pigments
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
    • A61K6/818—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising zirconium oxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
    • C04B2235/6585—Oxygen containing atmosphere, e.g. with changing oxygen pressures at an oxygen percentage above that of air
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6586—Processes characterised by the flow of gas
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/661—Multi-step sintering
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
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    • C04B2235/765—Tetragonal symmetry
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9646—Optical properties
    • C04B2235/9661—Colour
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    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32—Ceramic
    • C04B2237/34—Oxidic
    • C04B2237/345—Refractory metal oxides
    • C04B2237/348—Zirconia, hafnia, zirconates or hafnates
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    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/58—Forming a gradient in composition or in properties across the laminate or the joined articles

Definitions

  • the present invention relates to a process which, starting from an oxide ceramic material, enables the production of a dental restoration with excellent properties in a short time.
  • the invention also relates to the use of an oxide ceramic material for the preparation of a dental restoration by means of the process according to the invention.
  • Ceramic materials such as oxide ceramics are frequently used to fabricate fully anatomical dental restorations. They offer a high degree of clinical safety, are usually metal-free, can also be used for minimally invasive preparations and are very attractive in terms of price compared to other metal-free restorations. However, the numerous working steps that are usually required to fabricate such restorations are a disadvantage.
  • the restorations are usually milled or ground from presintered blanks, shaded if necessary, densely sintered by thermal treatment and finally further shaded, glazed and/or polished if necessary.
  • EP 2 098 188 A1 and corresponding U.S. Pat. No. 9,033,703, which US patent is incorporated by reference in its entirety, describe a dental furnace and a method for sintering dental materials, in which the furnace is heated to a presintering temperature of at least 1000° C. in a first heating period at a rapid heating rate of more than 50 K/min.
  • EP 2 101 133 A1 describes a sintering furnace and a process for sintering dental articles, in which the dental articles are moved along a sintering section and exposed to different temperatures. High heating rates of 300 K/min or more can be used in a first section.
  • WO 2015/091744 A1 and corresponding U.S. Ser. No. 10/939,980 which US patent is incorporated by reference in its entirety, describe a process for planning the sintering of a dental prosthesis part, in which a temperature profile for the heat treatment of the dental prosthesis part is automatically determined by means of a computer as a function of certain geometry and material parameters of the dental prosthesis part to be produced. A heating rate between 100 K/min and 400 K/min is used for the sintering of certain dental prosthesis parts.
  • WO 2011/020688 A1 describes a device for oxygen-free sintering of metal or ceramics in dental technology under inert gas.
  • EP 2 703 760 A1 describes a dental furnace for sintering a dental prosthesis, the heating chamber of which can be closed either by means of a conventional closing device such as a door or by means of an attachment with a vacuum container and can thus be used either for normal sintering or for vacuum sintering.
  • EP 3 659 548 A1 and corresponding US 2020170765 which US published application is incorporated by reference in its entirety, describe a process of manufacturing a dental restoration in which an oxide ceramic material is subjected to at least two heat treatments, the first heat treatment being carried out at a lower pressure than the second heat treatment.
  • the invention is therefore based on the problem of providing a process for the preparation of a dental restoration by which dental restorations with excellent mechanical and, in particular, optical properties can be produced in a short time by sintering oxide ceramic material.
  • cooling comprises (b1) a first cooling step with the cooling rate T1 and (b2) a second cooling step with the cooling rate T2 and wherein the absolute value of the cooling rate T2 is less than the absolute value of the cooling rate T1.
  • the process according to the invention allows very fast sintering of oxide ceramics to dental restorations, which have good mechanical properties and in particular a high density and at the same time can meet the high aesthetic requirements of dental restorations and imitate the optical properties of natural dental material in an excellent manner.
  • the oxide ceramic material used in step (a) is usually a non-densely sintered and in particular a presintered oxide ceramic material.
  • the oxide ceramic material used has a relative density in the range from 30 to 90%, in particular in the range from 40 to 80% and preferably in the range from 50 to 70%, in each case based on the true density of the oxide ceramic material.
  • the relative density is the ratio of the apparent density of the oxide ceramic material to the true density of the oxide ceramic material.
  • the apparent density of the oxide ceramic material can be determined by weighing it and determining its volume geometrically. The density is then calculated according to the known formula
  • the determination of the true density of the oxide ceramic material is carried out by grinding the oxide ceramic material to a powder with an average particle size of 10 to 30 ⁇ m, in particular 20 ⁇ m, based on the number of particles, and determining the density of the powder by means of a pycnometer.
  • the particle size can be determined, for example, with the CILAS® Particle Size Analyzer 1064 from Quantachrome GmbH & Co. KG using laser diffraction according to ISO 13320 (2009).
  • the cooling comprises
  • step (b2) in which the absolute value of the cooling rate T2 is smaller than the absolute values of the cooling rate T1 and optionally of the cooling rate T3, takes place in a temperature range from 1000 to 1500° C., preferably 1100 to 1400° C. and particularly preferably 1200 to 1300° C.
  • step (b2) the absolute value of cooling rate T2 is less than 60 K/min, preferably less than 50 K/min, more preferably less than 40 K/min, further preferably less than 25 K/min, even more preferably less than 10 K/min and most preferably less than 5 K/min.
  • step (b2) is carried out at a substantially constant temperature such that the cooling rate T2 is about 0 K/min.
  • Step (b2) can be carried out in particular for a duration of 1 to 20 min, preferably 1 to 10 min, more preferably 2 to 8 min, particularly preferably 3 to 7 min and most preferably 4 to 6 min.
  • the absolute value of the cooling rate T2 is smaller than the absolute values of the cooling rate T1 and optionally of the cooling rate T3.
  • the absolute value of the cooling rate T1 is at least 40 K/min, preferably at least 50 K/min and particularly preferably at least 60 K/min and is in particular in the range of 40 to 200 K/min, preferably 50 to 100 K/min and particularly preferably 60 to 80 K/min.
  • the absolute value of the cooling rate T3 is at least 40 K/min, preferably at least 50 K/min and particularly preferably at least 60 K/min and is in particular in the range of 40 to 200 K/min, preferably 50 to 100 K/min and particularly preferably 60 to 80 K/min.
  • the absolute values of the cooling rates T1 and T3 are each at least 40 K/min, preferably at least 50 K/min and particularly preferably at least 60 K/min and are in particular in the range from 40 to 200 K/min, preferably 50 to 100 K/min and particularly preferably 60 to 80 K/min.
  • the oxide ceramic material is preferably heated to a temperature which is in the range of 1100 to 1700° C., preferably in the range of 1300 to 1600° C., more preferably in the range of 1400 to 1550° C., and particularly preferably in the range of 1450 to 1500° C., and most preferably is about 1480° C. It is further preferred that the oxide ceramic material after carrying out step (a) has a relative density in the range of 90 to 97%, preferably in the range of 93 to 96% and particularly preferably a relative density of about 95%, in each case based on the true density of the oxide ceramic material.
  • the oxide ceramic material is heated in step (a) at a heating rate in the range of 5 to 500 K/min, preferably 50 to 250 K/min and particularly preferably 100 to 200 K/min.
  • the oxide ceramic material is first heated at a heating rate of 50 to 500 K/min, preferably 75 to 250 K/min and particularly preferably 100 to 200 K/min to a temperature which is 100 to 800 K, preferably 300 to 700 K and particularly preferably 500 to 600 K below the maximum temperature reached in step (a), and then further heated at a heating rate of 5 to 200 K/min, preferably 10 to 100 K/min and particularly preferably 25 to 50 K/min.
  • the oxide ceramic material is preferably cooled to a temperature which is in the range of 20 to 1300° C., preferably in the range of 100 to 1250° C., and particularly preferably in the range of 1000 to 1200° C. After reaching such a temperature, the oxide ceramic material can be removed from the heating chamber.
  • step (a) is particularly preferred in which the oxide ceramic material in step (a) is
  • step (a1) subjected to a first heat treatment, and (a2) subjected to a second heat treatment, wherein the heat treatment in step (a1) is carried out at a lower pressure than the heat treatment in step (a2).
  • the heat treatment in step (a1) is carried out at a pressure of less than 200 mbar, preferably less than 100 mbar and particularly preferably less than 50 mbar, and in particular at a pressure in the range from 0.1 to 200 mbar, preferably in the range from 1 to 150 mbar and particularly preferably in the range from 50 to 100 mbar.
  • This pressure can be set at ambient temperature before starting to heat the oxide ceramic material.
  • the oxide ceramic material may first be heated to a temperature above ambient temperature before the pressure defined for step (a) is adjusted.
  • This temperature is preferably in the range of 20 to 500° C., and in particular in the range of 25 to 100° C.
  • the oxide ceramic material is preferably further heated and held and sintered at a, preferably constant, temperature in the range of 1100 to 1700° C., in particular in the range of 1300 to 1600° C., preferably in the range of 1400 to 1550° C., more preferably in the range of 1450 to 1500° C. and most preferably at a temperature of about 1480° C.
  • the further heating is preferably carried out at a heating rate of 5 to 200 K/min, in particular 10 to 100 K/min and preferably 25 to 50 K/min.
  • the holding is preferably carried out for 1 to 60 minutes, in particular 5 to 30 minutes, preferably 10 to 25 minutes and particularly preferably 15 to 20 minutes.
  • the oxide ceramic material By holding at the corresponding temperature, the oxide ceramic material is typically densely sintered. Thereafter, the oxide ceramic material preferably has a relative density of at least 97%, in particular at least 98%, preferably at least 99% and most preferably at least 99.5%, in each case based on the true density of the oxide ceramic material.
  • the heat treatment in step (a2) is preferably carried out at a pressure greater than 500 mbar and in particular at ambient pressure.
  • the heat treatment in step (a2) is carried out in an oxygen-containing atmosphere.
  • air, oxygen-enriched air as well as oxygen can be considered as an oxygen-containing atmosphere.
  • the heating chamber used for the heat treatment can be filled with air and/or oxygen.
  • an oxygen-containing atmosphere preferably air, oxygen-enriched air or oxygen, flows discontinuously or preferably continuously through the heating chamber used for the heat treatment during step (a2), in particular at a flow rate of 0.1 to 50 l/min, preferably 1 to 10 l/min and particularly preferably 2 to 5 l/min.
  • the oxide ceramic material is heated in step (a1) to a temperature that is 0 to 500 K, in particular 10 to 250 K, preferably 50 to 150 K, and more preferably 75 to 100 K below the temperature or temperature range at which the oxide ceramic material is maintained in step (a2).
  • the oxide ceramic material obtained by the process according to the invention preferably has a number-average grain size in the range from 1 nm to 1000 nm, in particular from 10 nm to 800 nm and preferably from 100 nm to 600 nm.
  • the number-average grain size can be determined in particular by the line intersection method according to DIN EN 623-3 or ASTM E 112, wherein the value determined is used for conversion to the real number-average grain size in the three-dimensional microstructure according to M. I. Mendelson, J. Am. Ceram. Soc. 1969, 52(8), 443-446 by multiplying it by a proportionality constant of 1.56.
  • Oxide ceramic materials are generally highly crystalline ceramic materials based on oxide compounds and are having at most a very small proportion of glass phase.
  • Typical oxide ceramic materials are based on ZrO 2 , Al 2 O 3 , TiO 2 , MgO, combinations, solid solutions or composites thereof, in particular ZrO 2 /Al 2 O 3 (ZTA), Al 2 O 3 /ZrO 2 (ATZ) or ZrO 2 /spinel, with spinel preferably being Sr-spinel, Mg-spinel, La-spinel and/or Ce-spinel.
  • Oxide ceramic materials based on ZrO 2 and/or Al 2 O 3 are preferred according to the invention.
  • Oxide ceramic materials based on zirconium oxide and in particular based on polycrystalline tetragonal zirconium oxide (TZP) are particularly preferred. Even more preferred are oxide ceramic materials based on zirconium oxide in which the zirconium oxide is stabilized with Y 2 O 3 , La 2 O 3 , CeO 2 , MgO and/or CaO and is preferably stabilized with 2 to 12 mol %, in particular 3 to 6 mol %, of these oxides, based on the zirconium oxide content.
  • the oxide ceramic material is coloured.
  • this refers to an oxide ceramic material to which one or more colouring elements have been added.
  • suitable colouring elements are Fe, Mn, Cr, Pr, Tb, Er, Yb, Ce, Co, Ni, Nd, Cu and Bi.
  • the oxide ceramic material in particular comprises Fe.
  • the oxide ceramic material comprises at least two layers which differ in particular in their color.
  • colour and “coloured” refer to the colour, brightness and/or translucency of a material.
  • Translucency is the light transmission of a material, body or layer, i.e. the ratio of transmitted to incident light intensity.
  • Colors can also be characterized by the color coordinates L*, a* and b* in the L*a*b* color space or by a color code commonly used in the dental industry.
  • the L* value describes the brightness of a color with values from 0 (black) to 100 (white)
  • the a* value describes the green or red component of a color, where negative values represent green and positive values represent red
  • the b* value describes the blue or yellow component of a color, where negative values represent blue and positive values represent yellow.
  • Color differences can be expressed in the L*a*b* color space by the ⁇ E* value, which is calculated as follows:
  • ⁇ E * ⁇ (( ⁇ L *) 2 ( ⁇ a *) 2 ( ⁇ b *) 2 ).
  • color codes commonly used in the dental industry are Vitapan Classical® and Vita 3D Master®, both from VITA Zahnfabrik H. Rauter GmbH & Co. KG, and Chromascop® from Ivoclar Vivadent AG.
  • the translucency can be characterized by the contrast value CR, where 0% means completely transparent and 100% completely opaque.
  • the color coordinates L*, a* and b* are determined according to DIN 5033 and DIN 6174 and the translucency according to BS 5612.
  • the corresponding measurements can be carried out in particular by means of a spectrophotometer of the type CM-3700d (Konica-Minolta).
  • CM-3700d Konica-Minolta
  • specimens are used for the measurements which have been wet ground on both sides with diamond particles (particle size 15-20 ⁇ m) to obtain a final specimen thickness of 2.00 ⁇ 0.025 mm.
  • the color or colors of the dental restoration obtained according to the invention are in the range of the colors of natural teeth.
  • the dental restoration obtained according to the invention has an L* value in the range from 50 to 100, in particular in the range from 80 to 97, an a* value in the range from ⁇ 10 to 10, in particular in the range from ⁇ 1 to 5, a b* value in the range from 0 to 50, in particular in the range from 1 to 20, and/or a CR value in the range from 50 to 100%, in particular in the range from 75 to 99%.
  • the process according to the invention is particularly suitable for the preparation of dental restorations.
  • Particularly preferred dental restorations are bridges, inlays, onlays, crowns, veneers, facets and abutments.
  • the process according to the invention is particularly suitable for the preparation of dental restorations, in particular bridges, which comprise two or more members.
  • the invention also relates to the use of an oxide ceramic material for the preparation of a dental restoration, in which the oxide ceramic material is
  • cooling comprises (b1) a first cooling step with the cooling rate T1 and (b2) a second cooling step with the cooling rate T2 and wherein the absolute value of the cooling rate T2 is less than the absolute value of the cooling rate T1.
  • Test specimens with a diameter of 24 mm and a height of 2.9 mm were fabricated from a commercial zirconia-based oxide ceramic material containing 9.23 wt.-% Y 2 O 3 , 0.045 wt.-% Al 2 O 3 , and 0.25 wt.-% Fe 2 O 3 (Zpex smile yellow from the company Tosoh) by uniaxial pressing at a pressure of 150 MPa and heat treatment at 1000° C. for 2 hours.
  • test specimens were sintered in a sintering furnace with MoSi 2 heating element.
  • the test specimen was placed in the heating chamber of the sintering furnace at room temperature, the heating chamber was closed and a partial vacuum with a final pressure of about 50 to 100 mbar was created in the heating chamber.
  • the test specimen was heated at a heating rate of about 130 K/min to a temperature of about 900° C., then at a heating rate of about 50 K/min to a temperature of about 1220° C., and further at a heating rate of about 10 K/min to a temperature of about 1400° C.
  • the heating chamber was flooded with fresh air and then continuously flowed with fresh air at a flow rate of about 2.2 l/min while the test specimen was further heated to a temperature of 1480° C. at a heating rate of about 10 K/min and held at this temperature for about 17 minutes. Thereafter, the test specimen was cooled to a temperature T at a cooling rate of about 70 K/min according to Table 1, held at this temperature for a period of t minutes, and then further cooled to a temperature of about 1200° C. at a cooling rate of about 70 K/min. The heating chamber was then opened. The total duration of the sintering process was between 64 and 66 min.
  • Example 1A was repeated, but the specimen was cooled from 1480° C. to 1200° C. at a continuous cooling rate of about 70 K/min without interruption. The total duration of the sintering process was about 60 min.
  • Example 1A was repeated, but using a slow sintering process.
  • the test specimen was heated at a heating rate of about 10 K/min to a temperature of about 900° C., held at this temperature for 30 min, further heated at a heating rate of about 3 K/min to a temperature of about 1500° C. and held at this temperature for about 120 min. Thereafter, the test specimen was cooled to 900° C. at a cooling rate of about 10 K/min and further cooled to 300° C. at a cooling rate of about 8 K/min. The heating chamber was then opened. The total duration of the sintering process was about 575 min.
  • Examples 1A-H The CR values and color coordinates of the oxide ceramic materials obtained in Examples 1A-H are shown in Table 1. It can be seen that Examples 1A to 1F according to the invention show significantly higher a* values and b* values compared to Example 1G, which was also obtained using a rapid sintering process, and that the a* values are consistently in the positive range. As a result, these examples are more suitable for imitating the color properties of natural dental material. At the same time, the sintering process used for examples 1A to 1F according to the invention requires only about one tenth of the duration of the slow sintering process according to example 1H.

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